WO2017080473A1 - Membrane tubulaire de fibres ultrafines de polytétrafluoroéthylène - Google Patents
Membrane tubulaire de fibres ultrafines de polytétrafluoroéthylène Download PDFInfo
- Publication number
- WO2017080473A1 WO2017080473A1 PCT/CN2016/105274 CN2016105274W WO2017080473A1 WO 2017080473 A1 WO2017080473 A1 WO 2017080473A1 CN 2016105274 W CN2016105274 W CN 2016105274W WO 2017080473 A1 WO2017080473 A1 WO 2017080473A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- cavity
- mass
- fiber membrane
- porous material
- polytetrafluoroethylene
- Prior art date
Links
- 239000012528 membrane Substances 0.000 title claims abstract description 51
- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 47
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 47
- -1 Polytetrafluoroethylene Polymers 0.000 title claims abstract description 44
- 229920001410 Microfiber Polymers 0.000 title abstract description 3
- 239000011148 porous material Substances 0.000 claims abstract description 78
- 239000000835 fiber Substances 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004821 distillation Methods 0.000 claims description 15
- 238000009827 uniform distribution Methods 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000002253 acid Substances 0.000 description 10
- 230000004907 flux Effects 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 238000001523 electrospinning Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229920001661 Chitosan Polymers 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000012510 hollow fiber Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/364—Membrane distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/36—Polytetrafluoroethene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
Definitions
- the present invention relates to a porous material, in particular a polytetrafluoroethylene fiber membrane, which is particularly suitable for membrane distillation.
- porous material A solid containing a certain number of pores is called a porous material and is a material that forms a network structure by through or closed pores.
- porous materials Compared with continuous medium materials, porous materials generally have the advantages of low relative density, high specific strength, high specific surface area, light weight, sound insulation, heat insulation and good permeability.
- the porous material can be divided into microporous (pore size less than 2 nm) material, mesoporous (pore size 2-50 nm) material and macroporous (pore size greater than 50 nm) material.
- Porous materials are classified according to their materials and can be classified into metal porous materials and non-metallic porous materials.
- Non-metallic porous materials generally have the characteristics of large specific surface area, small density, small thermal conductivity, small relative density, and high porosity. They are used in catalysts (including carriers), adsorbents, heat preservation, heat insulation, sewage and waste gas treatment, filtration of liquids, and Gas (even bacteria), lightweight building materials, environmental protection, soil improvement, chemical industry and other fields have broad application prospects.
- the polytetrafluoroethylene porous membrane material has a wide application range due to its temperature stability, chemical stability, electrical insulation, flame retardancy and self-lubricating properties. However, due to the randomness and irregularity of the pore structure, it still cannot satisfy many application properties.
- the porous material itself needs to be uniform, its pore size and pore distribution are uniform, so that the performance is uniform, but in fact, many porous materials do not meet this requirement, and their uniformity complements; although some materials claim to be self-proclaimed Achieve higher uniformity, but its uniformity is still uniformity on a large volume scale. If it is measured by a small volume scale, for example, if a plurality of three-dimensional bodies having a volume of not more than one cubic centimeter are taken on the material, respectively, The quality, the degree of uniformity is still very large, thus causing various properties of the polytetrafluoroethylene porous membrane material such as strength, elastic modulus, flux and the like, which seriously affect its function.
- the object of the present invention is to provide a polytetrafluoroethylene fiber membrane which is structurally suitable, controllable and highly uniform.
- the object of the invention is achieved by the following measures:
- a polytetrafluoroethylene ultrafine fiber membrane comprising a body of polytetrafluoroethylene material, a polytetrafluoroethylene fiber, a fiber diameter of 30-200 nm, a body having a pore size of 10 nm to 1000 nm, and a three-dimensional space surrounding the cavity
- the cavity wall is formed with uniform distribution, and each cavity is three-dimensionally penetrated.
- the uniform distribution of the cavity means that each cavity is uniformly distributed under arbitrary unit volume on the porous material; porosity is ⁇ 75%
- the tensile strength is 15 N/mm 2 or more, and the water pressure resistance is 3 kg/cm 2 or more.
- the polytetrafluoroethylene fiber membrane has a cavity having a pore diameter of 30 to 1000 nm and a cavity wall formed in a three-dimensional space around the cavity, and a lower cavity of 10 to 100 nm is disposed on the cavity wall, and each cavity of each cavity is three-dimensionally Through and holes
- the cavities are also connected to each other; the cavities are uniformly distributed, and the uniformity of the cavities means that the cavities are uniformly distributed under arbitrary unit volume on the porous material.
- the above unit-level volume means a cubic centimeter-level or cubic millimeter-level or smaller unit-level volume.
- the uniform distribution of the above-mentioned cavities means that each of the three-dimensional bodies having a volume of not more than one cubic centimeter and the same size on the porous material is substantially equivalent in mass.
- the above-mentioned mass is substantially equivalent to a plurality of three-dimensional bodies having a volume of not more than one cubic centimeter and the same size, which are respectively referred to as a mass, and an average value of their masses is obtained, and any three-dimensional mass is relatively
- the absolute value of the deviation from the mass average is not more than 4% of the average of the three-dimensional body mass.
- the three-dimensional bodies of the same size having a volume of not more than one cubic millimeter on the multi-stage material are substantially equivalent in mass.
- the mass is substantially equivalent to a plurality of three-dimensional bodies of the same size having a volume of not more than one cubic millimeter on the porous material, respectively referred to as masses, and an average value of their masses is obtained, and any three-dimensional mass is obtained.
- the absolute value of the deviation from the mass average is not more than 4% of the average of the three-dimensional body mass.
- the polytetrafluoroethylene fiber membrane is composed of a multi-stage porous material
- the body is a cavity which is classified by a material pore size, and a cavity wall which surrounds the cavity in a three-dimensional space, and a lower cavity is arranged on the cavity wall, and each The stages of the cavities are each three-dimensionally penetrated and the cavities of the stages are also connected to each other.
- the next level of porous material constitutes the wall of the cavity of the upper stage.
- the cavity wall of the upper cavity is composed of a multi-stage porous material of its lower stage or a composite of porous materials of the lower stage, so that the material can meet specific functional requirements.
- each stage of the porous material of the material body is self-contained as a continuous structure.
- the maximum outer boundary of each level of porous material is comparable to the entire material body space boundary. That is, each grade of porous material can exist in the bulk as a first-order independent porous material, and has its own physical and chemical properties. Such a structure can make the physical and chemical properties of the porous materials of different levels different, and have different physical and chemical properties in the entire space of the relatively fixed materials, and better meet various functional requirements.
- the present invention provides a polytetrafluoroethylene fiber membrane having a porous structure, and the structural form thereof is clarified, and the hierarchical structure of the pore cavity and the uniform structure thereof can satisfy various functional requirements.
- the present invention provides a specific and clear measurement method for the uniform distribution of the pores of the polytetrafluoroethylene fiber membrane, and clarifies that the pore distribution uniformity of the porous material and its multi-stage structure is measured on the scale of the small unit volume.
- Such a porous structure is highly uniform, thereby ensuring uniformity of the properties of the porous material.
- the polytetrafluoroethylene fiber membrane of the present invention is three-dimensionally penetrated, including three-dimensional communication of each level of holes, and three-dimensional through-holes of each level, and good penetration, and can fully meet the functional requirements of the material.
- the polytetrafluoroethylene fiber membrane of the present invention is a hydrophobic surface having a multistage roughness structure.
- the surface water contact angle can reach 160° or more.
- Polytetrafluoroethylene porous fiber membrane such as pore distribution, hierarchical structure, porosity, pore shape and other structural characteristics, processes and the like are related to mechanical properties such as mechanical strength and water pressure resistance, and the polytetrafluoroethylene fiber membrane of the present invention No support, stable shape, controllable thickness, applied to membrane distillation process, flux >42L/m 2 ⁇ h, rejection rate above 99.8%, tensile strength up to 30N/mm 2 or more, water pressure resistance 5kg/cm 2 the above.
- the polytetrafluoroethylene fiber membrane of the present invention may be a film of different shapes and specifications such as a flat plate type, a tubular type, a hollow fiber type or a roll type, without support, and has a stable shape and a controllable thickness.
- the polytetrafluoroethylene fiber membrane of the invention has a secondary pore structure, wherein the cavity wall of the first-stage cavity uniformly distributed and interpenetrating has a second-stage cavity uniformly distributed and mutually penetrating, and the two-stage hole The two are also connected to each other, and the through-holes are three-dimensionally penetrated.
- Each level of porous material of the material body is self-contained as a continuous structure.
- the total effective porosity is 75%
- the fiber diameter is 150 ⁇ 20 nm
- the macroporous average pore diameter is 0.45 ⁇ m
- the preparation method of the polytetrafluoroethylene porous material is:
- a polytetrafluoroethylene emulsion having a solid content of 60%, a chitosan having a particle size of 30 nm, a 5% (mass ratio) polyacrylic acid solution, and a 20 wt% starch emulsion are uniformly mixed according to the mass of 50:25:4:4. Ratio, formulated into a spinning solution;
- the precursor film is wound up to 5 layers on a cylindrical support mold, sent to a tube furnace for sintering in a vacuum or a protective atmosphere, and sintering is sequentially sintered by program temperature control, and is heated from room temperature at a rate of 5 ° C/min.
- Incubate at 160 ° C for 80 min at 160 ° C; ramp up to 280 ° C at 5 ° C / min, hold at 280 ° C for 60 min; ramp to 360 ° C at 2 ° C / min, hold at 360 ° C for 20 min; at 6 ° C /
- the rate of min was raised to 400 ° C and incubated at 400 ° C for 60 min.
- the PTFE fiber membrane does not need to be supported, has stable shape and controllable thickness, and can be used for gas-liquid separation and liquid-liquid separation to achieve precise grading filtration, for example, it is suitable for filtering of two-component or multi-component gas (liquid) body,
- the flux is large, the rejection rate is high, and it is not easy to be polluted (such as the contamination of the multi-liquid immersion membrane), and has the advantages of high efficiency and long-term efficiency.
- the film water contact angle was 168°; the tensile strength was 30 N/mm 2 , and the water pressure resistance was 5 kg/cm 2 .
- Volatile alcohol/acid separation factor [alcohol / acid mass fraction in distillate ⁇ (1 - raw material liquid alcohol / acid mass fraction)] ⁇ [raw material liquid alcohol / acid mass fraction ⁇ (1- distillate alcohol / acid mass fraction)] can reach 10 the above.
- the polytetrafluoroethylene fiber membrane of the invention has a three-stage pore structure, wherein the cavity wall of the first-stage cavity uniformly distributed and interpenetrating has a second-stage cavity uniformly distributed and mutually penetrating, and the two-stage hole The two are also connected to each other, and the through-holes are three-dimensionally penetrated.
- Each level of porous material of the material body is self-contained as a continuous structure.
- the total effective porosity is 85%, the fiber diameter is 180 ⁇ 20 nm, the macroporous average pore diameter is 800 nm, and there are average secondary pores of 60 nm in the cavity wall of the macropores, and there is an average on the pore walls of the second-stage pores.
- a third-stage hole having a pore diameter of 10 nm.
- the preparation method of the polytetrafluoroethylene porous material is:
- the precursor film is wound up to 5 layers to a 2 mm diameter cylindrical support mold, sent to a tube furnace for sintering in a vacuum or a protective atmosphere, and sintered by program temperature control and continuous sintering at a rate of 5 ° C / min.
- the temperature is raised to 160 ° C at room temperature, 80 min at 160 ° C; the temperature is raised to 290 ° C at 5 ° C / min, incubated at 290 ° C for 60 min; the temperature is raised to 360 ° C at 2 ° C / min, and kept at 360 ° C for 20 min;
- the rate of °C/min is raised to 400 ° C, and kept at 400 ° C for 60 min;
- the program was temperature-controlled and cooled, and a porous polytetrafluoroethylene hollow fiber membrane having a three-stage pore structure was obtained according to a conventional technique, and the thickness was 168 ⁇ m, and the fiber membrane diameter was 2 mm.
- the PTFE fiber membrane does not need to be supported, has stable shape and controllable thickness, and can be used for gas-liquid separation and liquid-liquid separation to achieve precise grading filtration, for example, it is suitable for filtering of two-component or multi-component gas (liquid) body,
- the flux is large, the rejection rate is high, and it is not easy to be polluted (such as the contamination of the multi-liquid immersion membrane), and has the advantages of high efficiency and long-term efficiency.
- the film water contact angle was 170°; the tensile strength was 28 N/mm 2 , and the water pressure resistance was 7 kg/cm 2 .
- Alcohol/acid separation factor [alcohol/acid mass fraction in distillate ⁇ (1 - raw material liquid ethanol mass fraction)] ⁇ [raw material liquid alcohol / acid mass fraction ⁇ (1-distillate alcohol / acid mass fraction)] Can reach more than 10.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Artificial Filaments (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
La présente invention concerne une membrane tubulaire de fibres ultrafines de polytétrafluoroéthylène comprenant un corps de matériau de polytétrafluoroéthylène; le polytétrafluoroéthylène a une forme de fibre et la fibre a un diamètre de 30 à 200 nm; le corps comporte des cavités de pore ayant un diamètre de 10 à 1000 nm et des parois de cavité formées par des espaces tridimensionnels entourant les cavités de pore; les cavités de pore sont uniformément distribuées et chaque cavité de pore est ouverte de façon tridimensionnelle; la porosité est ≥ 75 %, la résistance à la traction est de 15 N/mm² ou plus, et la résistance à la pression d'eau est supérieure à 3 kg/cm² ou plus.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510767099.2 | 2015-11-11 | ||
CN201510767099.2A CN106669457B (zh) | 2015-11-11 | 2015-11-11 | 一种聚四氟乙烯超细纤维膜 |
Publications (1)
Publication Number | Publication Date |
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WO2017080473A1 true WO2017080473A1 (fr) | 2017-05-18 |
Family
ID=58694581
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/CN2016/105274 WO2017080473A1 (fr) | 2015-11-11 | 2016-11-10 | Membrane tubulaire de fibres ultrafines de polytétrafluoroéthylène |
Country Status (2)
Country | Link |
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CN (1) | CN106669457B (fr) |
WO (1) | WO2017080473A1 (fr) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109550401A (zh) * | 2017-09-26 | 2019-04-02 | 重庆润泽医药有限公司 | 一种膜蒸馏用复合材料 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101530750A (zh) * | 2009-04-20 | 2009-09-16 | 浙江理工大学 | 聚四氟乙烯超细纤维多孔膜的制备方法 |
CN101543734A (zh) * | 2008-11-21 | 2009-09-30 | 任正善 | 一种聚四氟乙烯纳米纤维膜及制备方法 |
CN102151493A (zh) * | 2011-03-18 | 2011-08-17 | 上腾新材料科技(苏州)有限公司 | 一种纳米级聚四氟乙烯微孔膜的制备方法 |
WO2013005430A1 (fr) * | 2011-07-05 | 2013-01-10 | 日東電工株式会社 | Film poreux de polytétrafluoroéthylène et matériau filtrant pour filtre à air |
CN103191653A (zh) * | 2012-01-10 | 2013-07-10 | 杭州科百特过滤器材有限公司 | 一种形成非对称聚四氟乙烯多孔膜的方法 |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4659241B2 (ja) * | 2001-03-19 | 2011-03-30 | ジャパンゴアテックス株式会社 | ポリテトラフルオロエチレン膜及びその製造方法 |
CN102941025A (zh) * | 2012-11-20 | 2013-02-27 | 浙江理工大学 | 一种膜蒸馏用聚四氟乙烯中空纤维膜的制备方法 |
CN107537327B (zh) * | 2014-03-13 | 2020-01-03 | 成都百途医药科技有限公司 | 一种聚四氟乙烯膜及其制备方法 |
CN103894077B (zh) * | 2014-04-10 | 2016-02-24 | 江南大学 | 一种多维度孔隙结构复合过滤膜及其制备方法 |
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2015
- 2015-11-11 CN CN201510767099.2A patent/CN106669457B/zh active Active
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2016
- 2016-11-10 WO PCT/CN2016/105274 patent/WO2017080473A1/fr active Application Filing
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101543734A (zh) * | 2008-11-21 | 2009-09-30 | 任正善 | 一种聚四氟乙烯纳米纤维膜及制备方法 |
CN101530750A (zh) * | 2009-04-20 | 2009-09-16 | 浙江理工大学 | 聚四氟乙烯超细纤维多孔膜的制备方法 |
CN102151493A (zh) * | 2011-03-18 | 2011-08-17 | 上腾新材料科技(苏州)有限公司 | 一种纳米级聚四氟乙烯微孔膜的制备方法 |
WO2013005430A1 (fr) * | 2011-07-05 | 2013-01-10 | 日東電工株式会社 | Film poreux de polytétrafluoroéthylène et matériau filtrant pour filtre à air |
CN103191653A (zh) * | 2012-01-10 | 2013-07-10 | 杭州科百特过滤器材有限公司 | 一种形成非对称聚四氟乙烯多孔膜的方法 |
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Publication number | Publication date |
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CN106669457B (zh) | 2020-11-20 |
CN106669457A (zh) | 2017-05-17 |
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